참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-Bromo-2-methylpropionyl bromide | HCID 88685 | — |
| 반응물 | 2-(2,2-Dimethoxyethoxy)ethan-1-ol | HCID 19736275 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Bromo-2-methyl-propionic acid 2-(2,2-dimethoxy-ethoxy)-ethyl ester | HCID 59391597 | — |
반응 단계
A solution of 2-(2,2-dimethoxy-ethoxy)-ethanol (2.20 g, 14.6 mmol) from Example 9 in dry triethylamine (3.0 mL, 21 mmol) and dry methylene chloride (30 mL) was stirred at 0° C. 2-bromo-2-methylpropionyl bromide (1.7 mL, 14 mmol) methylene chloride (10 mL) was then added to the alcohol over a 15 minute period. The reaction mixture was warmed to room temperature and stirred overnight. The reaction mixture was filtered, the filtrate was washed with saturated sodium bicarbonate, and dried with magnesium sulfate. The solvent was removed and the yellow oil purified by column chromatography. 1H NMR (300 MHz, CDCl3): δ=1.78 (s, 6H), 3.31 (s, 6H), 3.49 (d, 2H), 3.68 (t, 2H), 4.25 (t, 2H), 4.46 (t, 1H) 13C NMR (300 MHz, CDCl3): δ=31.23, 55.85, 56.15, 65.58, 69.55, 71.44, 103.09, 172.07.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08846021B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-16ef7506915c4bbc8e3d335a930919f5 |
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| 출처 메모 | uspto-grants-2014_09 |
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